Application Compendium - Agilent Technologies

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Author Frank Higgins and Alan Rein Agilent Technologies Danbury, CT, USA Quantitative analysis of copolymers using the Cary 630 FTIR spectrometer Application note Materials testing and research Introduction FTIR spectrometers employing attenuated total refl ectance (ATR) sampling interfaces are a proven and powerful tool for the analysis of polymeric materials. Because of its unique combination of features and classleading performance, the new Agilent Cary 630 FTIR spectrometer makes quantitative analysis of polymers especially fast and easy. In this application note, the amount of key components in two important copolymeric materials are measured — the styrene content in styrene butadiene rubber (SBR) and the ratio of polyethylene to vinyl acetate in polyethylene vinyl acetate (PEVA) polymer. The Cary 630 FTIR equipped with its single refl ection Diamond ATR sampling accessory (Figure 1) is used for these measurements.
Figure 1. Agilent Cary 630 FTIR spectrometer equipped with single refl ection Diamond ATR sampling accessory Styrene concentration in SBR polymer Styrene butadiene rubber (SBR) is the most common synthetic rubber material and its main use is in the manufacture of tires, which accounts for nearly 70% of its production. The properties of SBR rubber can be altered by varying the ratio of styrene to butadiene monomers in the manufacturing process. The normal ratio is 3:1 butadiene to styrene (25% styrene). Higher styrene concentrations make the material harder, but less elastic. Most performance industries, such as racing tires and specialty military applications, are requiring more consistent SBR product, which drives the need for better quality assurance and control by both end users and manufacturers. The measurement of a polymer sample by the Cary 630 FTIR equipped with an ATR accessory is extremely straightforward. The polymer material is placed on the diamond crystal and the sample pressure press is rotated downward until adequate pressure is placed on the sample to observe a spectrum in the Cary 630’s realtime analysis MicroLab FTIR software (Figure 2). The real-time analysis mode provides instantaneous spectral update and makes it easy for even novice users to get highly repeatable results. The sample press on the Cary 630 is designed so that it cannot be over-tightened, thus protecting the diamond crystal against over-pressure. Figure 2. Polymer is placed directly on ATR sampling accessory. Uniform, constant pressure is provided by the sample press, ensuring that high quality spectra are obtained. Real-time analysis software provides an immediate indicator of spectral quality To develop a quantitative FTIR method, four commercial SBR calibration standards, with polystyrene concentrations of 0%, 5%, 23%, and 45%, were measured in triplicate using the Cary 630 FTIR. The spectra reveal the expected polystyrene (PS) absorbance bands (Figure 3) at 699 cm -1 , 759 cm -1 , and a weaker band at 1031 cm -1 . Spectral bands at 911 cm -1 , 964 cm -1 , and 995 cm -1 arise from unsaturations (vinyl and trans CH wag) in polybutadiene, which decrease as the PS bands increase. The exception is the pure polybutadiene, which has far more cis unsaturations relative to the other polymers, since it is not cross-linked and in liquid form. The PS absorbance bands appear to follow Beer’s Law by increasing proportionately with concentration, and therefore are excellent candidates for quantitative analysis. The plot of the peak height absorbance for the strongest IR band of PS at 699 cm -1 as a function of concentration indicates great linearity and a strong correlation coeffi cient of R 2 =0.999 in the calibration (Figure 4). Using the linear regression slope and offset from this calibration, a method is added to the MicroLab FTIR software that enables the polystyrene percentage in an unknown sample to be automatically displayed. The limit of detection for the quantitative analysis of PS in SBR is 0.09%, calculated as three times the standard deviation of the 0% replicate data (StDev= 0.03% PS). 2
Page 1 and 2: MATERIALS TESTING AND RESEARCH SOLU
Page 3 and 4: When accuracy and reliability in me
Page 5: AGILENT TECHNOLOGIES APPLICATIONS F
Page 9 and 10: The calibration samples were measur
Page 11 and 12: Author Frank Higgins Agilent Techno
Page 13 and 14: Figure 1. The overlaid aliphatic be
Page 15 and 16: Author John Seelenbinder Agilent Te
Page 17 and 18: Figure 3. Sample is lightly pressed
Page 19 and 20: Author Dr. Mustafa Kansiz Agilent T
Page 21 and 22: microscopy provides for a factor of
Page 23 and 24: Standard ATR IR Image No Pressure (
Page 25 and 26: A visual inspection of the sample u
Page 27 and 28: Experimental Instrumentation To per
Page 29 and 30: Authors Jonah Kirkwood † and Must
Page 31 and 32: Spectra were collected from each lo
Page 33 and 34: Infrared mapping allows for multipl
Page 35 and 36: The spectra in Figure 2 are visuall
Page 37 and 38: Conclusion Agilent‟s Cary 610 FTI
Page 39 and 40: Authors Dr. Wayne Collins*, John Se
Page 41 and 42: The calibration curve obtained for
Page 43 and 44: Conclusion Select ‘Peak Ratio’
Page 45 and 46: Summary This method describes a pro
Page 47 and 48: Method configuration To determine t
Page 49 and 50: Authors Dr. Wayne Collins*, John Se
Page 51 and 52: The calibration curve for the deter
Page 53 and 54: Figure 6. The MicroLab PC FTIR soft
Page 55 and 56: Summary An analytically representat
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Figure 3. The Irganox 1010 peak are
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Authors Dr. Wayne Collins*, John Se
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The calibration curve and equation
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Select ‘Peak Ratio’ - from the
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Summary An analytically representat
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Figure 3. The GMS peak height absor
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Advanced Atomic Force Microscopy: E
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signal) image indicating the overwh
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A dependence of surface potential o
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A B C Figure 6A-C. The topography (
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A B Figure 10A-C. The topography (A
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KFM with AM-FM operation in the int
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ibbons is only slightly different f
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References 1. G. Binnig, C.F. Quate
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Figure 1. AFM topographic image of
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100nm 100nm 350nm 100nm Figure 3. A
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to perfect hexagonal patterns, whic
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Single-pass KFM studies have been k
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images due to the difference of the
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0.5 V) of the nanowires. Additional
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appeared in the topography image. T
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of PSS component. TEM studies of mo
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Atomic Force Microscopy Studies in
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on graphite and MoS2 are shown in F
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A B C D Scan size: 5 µm. Scan size
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images of PEDOT:PSS blend, (PEDOT -
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Young’s Modulus of Dielectric ‘
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Figure 3. Young’s modulus as a fu
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Nanoindentation, Scratch, and Eleva
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The samples listed as “D” sampl
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Figure 6. Elastic modulus results f
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Figure 11. Elastic modulus results
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Sample B Figure 16. Scratch curves
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Conclusions Nanoindentation and scr
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measurement technique has been expl
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References 1. J.L. Hay, “Using In
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Theory The complex shear modulus (G
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References 1. Jain, S.K., Bhattacha
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LCCC relies on carrying out isocrat
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log Mp 5 4.6 4.2 3.8 0.5 15% Water
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Authors Wei Luan and Chunxiao Wang
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Table 1. Chemical Information of An
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Injection Volume Influence of Real
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translator into three modes on diff
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To identify the matrix influence on
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Authors Chun-Xiao Wang and Wei Luan
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Table 1. Polymer Additives in ASTM
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1 2 3 4 5 1 Tinuvin P 2 BHT 3 BHEB
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1 Tinuvin P 2 BHT 3 BHEB 4 Isonox 1
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Authors Edgar Naegele Agilent Techn
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Results and discussion To meet the
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Authors Melissa Dunkle, Gerd Vanhoe
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Experimental The analyses were perf
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Repeatability of the SFC/MS analysi
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Conclusion The combination of the A
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Introduction Phthalates form a grou
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The analytical method was applied t
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Introduction Bisphenol A (BPA) is a
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Preparation of standards BPA and BP
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Limit of Detection (LOD) and Limit
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Sample analysis The content of BPA
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The calibration for BPA and BPF, wh
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Author Stephen Ball Agilent Technol
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Results and discussion By operating
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Introduction The wavelength of UV r
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LC parameters Premixed solutions of
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Linearity A linearity study was per
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References 1. Dr. James H. Gibson,
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Instrumentation Columns: 2 x PLgel
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Authors Greg Saunders and Ben MacCr
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Authors Greg Saunders, Ben MacCreat
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Author Greg Saunders Agilent Techno
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Figure 5. Universal calibration cur
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Methods and Materials Conditions Co
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Materials and Methods A column set
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